US8203014B2 - Fractionation processes and devices for oils and fats - Google Patents

Fractionation processes and devices for oils and fats Download PDF

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US8203014B2
US8203014B2 US12/175,837 US17583708A US8203014B2 US 8203014 B2 US8203014 B2 US 8203014B2 US 17583708 A US17583708 A US 17583708A US 8203014 B2 US8203014 B2 US 8203014B2
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agitator
edible oils
fractionation process
fats
cooling
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US20090264667A1 (en
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Marc Kellens
Marc Hendrix
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De Smet Engineering NV SA
Desmet Belgium NV
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/44—Mixers with shaking, oscillating, or vibrating mechanisms with stirrers performing an oscillatory, vibratory or shaking movement
    • B01F31/441—Mixers with shaking, oscillating, or vibrating mechanisms with stirrers performing an oscillatory, vibratory or shaking movement performing a rectilinear reciprocating movement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/44—Mixers with shaking, oscillating, or vibrating mechanisms with stirrers performing an oscillatory, vibratory or shaking movement
    • B01F31/445—Mixers with shaking, oscillating, or vibrating mechanisms with stirrers performing an oscillatory, vibratory or shaking movement performing an oscillatory movement about an axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/44—Mixers with shaking, oscillating, or vibrating mechanisms with stirrers performing an oscillatory, vibratory or shaking movement
    • B01F31/449—Stirrers constructions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/93—Heating or cooling systems arranged inside the receptacle
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
    • C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F2035/98—Cooling

Definitions

  • the invention relates to fractional crystallization processes for oils and fats that aim at producing crystal slurries as well as to the crystallizers to be used in said crystallization processes.
  • fractional crystallization processes are regularly used to purify intermediate products and/or to isolate fractions having more desirable properties than their starting materials.
  • These starting materials can thereto be dissolved in a solvent to provide a solution that is then subjected to a fractional crystallization process. They can also be melted whereupon the melt is then partially crystallised.
  • the temperature of the solution or melt is lowered causing the solution or melt to become supersaturated and generate crystal nuclei. On further cooling, these nuclei grow into macroscopic crystals and form a crystal slurry.
  • This slurry is then subjected to a separation process which can be a continuous process using a drum filter, a continuous band filter, a sieve centrifuge or a decanter, or it can be a discontinuous separation process employing a filter press such as a plate and frame or a membrane filter press.
  • a filter press such as a plate and frame or a membrane filter press.
  • membrane press filters leave relatively little interstitial oil between the fat crystals and thus generate a relatively pure filter cake.
  • Other ways of achieving same involve using a solvent, which will dilute the interstitial oil, and especially washing the filter cake with clean solvent to dilute the interstitial solution even further. So whereas for the fractionation of edible oils and fats the so-called ‘dry fractionation process’ is generally preferred since it does not involve the use of highly inflammable solvents such as acetone or hexane, some products can only be obtained by using solvents during their fractional crystallization.
  • the fat to be fractionated is melted and then cooled in a crystallizer to produce a slurry of fat crystals in its mother liquor. This slurry is then separated into a filtrate that is commonly referred to as the ‘olein fraction’ and a filter cake that is called the ‘stearin fraction’.
  • the properties of the olein mainly depend upon the final crystallization temperature whereas the properties of the stearin fraction depend only slightly on this temperature but strongly on its olein content.
  • a batch crystallization process is generally preferred despite the fact that a continuous process is likely to be considerably cheaper.
  • Such batch processes allow of better control of the crystallization process parameters such as temperature and intensity of agitation.
  • such batch processes have the advantage over continuous processes in that the temperature of the batch crystallizer is raised above the melting point of the feedstock during each batch cycle. Accordingly, any crystal deposits on the crystallizer walls or cooling elements will be removed by being melted and no special wipers to clean these surfaces such as for instance described in U.S. Pat. No. 6,355,218 are needed.
  • a simple batch crystallization vessel used for the dry fractionation of edible oils and fats is the so-called “tubular crystallizer”.
  • This is a tall, cylindrical, double-walled vessel fitted with a central, axial agitator. Heat transfer is through the vessel wall and to ascertain a cooling surface of e.g. 7 m 2 per m 3 crystallizer volume, the diameter of such tubular crystallizers has to be limited to 0.6 m at most. Since agitators that are longer than 5 m would require an extra sturdy execution, the volume of this type of crystallizer is in practice limited to approximately 1.4 m 3 ; it is therefore mainly used for low-volume specialty fats, and less for bulk products such as palm oil.
  • a substantial increase in cooling surface per unit volume of oil has been realised in a crystallizer comprising concentric annular crystallization compartments that are separated by concentric, annular, double-walled cooling elements.
  • this type of crystallizer also exhibits an increased heat transfer coefficient of about 120-170 W/m 2 K presumably because the agitator blades move very close to the heat exchange surfaces.
  • this type of crystallizer is complex in construction and therefore expensive to build. Because the agitator blades are mounted on spokes connected to a central agitator shaft and move inside the annular compartments, these must be perfectly circular to prevent the blades from scraping the walls. Besides, including a labyrinth inside the double-walled cooling elements is not easy.
  • DE 19520675A1 discloses a process for crystallizing substances by cooling of a substance-containing liquid medium in a crystallizer, in particular for crystallizing organic fats from a melt, in which within the crystallizer at least one cooling element is provided for cooling the liquid medium and in which a relative motion is generated between the medium and the cooling element, characterized in that the medium is essentially static relative to a wall of the crystallizer and that the cooling element is subdivided into a plurality of tubular heat transfer elements, which move in closed paths and that all the heat transfer elements are moved essentially with the same speed relative to the medium.
  • DE 19520675A1 further discloses an apparatus in which the cooling unit is moved in relation to the wall of the crystallizer, through a coupling to a drive shaft and the coupling acts as a movement transmission to convert the central rotation of the drive shaft into an off-centre cooling element movement.
  • BE 877,839A relates to agitated heat exchangers for crystallised syrups. It discloses a vertical cylindrical vessel comprising a heat exchanger spirally arranged in a horizontal plane and to which is imparted a vertical downward and upward motion, and states that this construction allows for a better agitation than that obtained by means of a disc or a rotative blade.
  • DE 552,532 discloses a crystallization vessel wherein a cooling hollow body and a drive are suspended.
  • the drive imparts to the cooling hollow body a jerky vertical motion or a pendular motion around an axis in a horizontal direction.
  • GB 2,100,613A discloses producing a metallic slurry in which a metallic material is agitated by a reciprocating agitator.
  • the agitator is a plate or disc and is reciprocated in a direction substantially perpendicular to its major plane.
  • JP 07-284,643A discloses an agitated vessel for fishery product, said vessel comprising a plate impeller freely detachably hung from a rectilinearly reciprocating slider, wherein the impeller is inclined to the moving direction of said slider.
  • JP 2002-210,399A teaches preventing sedimentation of a solid content in a coating liquid filled in a stirred tank by horizontally reciprocally moving a water-feed panel arranged within said tank, said panel comprising a bent blade material bent to a V-shaped cross section and a bent blade material bent to a reverse V-shaped cross section; in this embodiment, the agitating blades are inclined to the moving direction.
  • a crystallizer comprising a crystallization vessel ( 1 , 2 ), an agitator or agitator assembly, and a drive, wherein said drive provides said agitator or agitator assembly with an oscillating motion (e.g. a reciprocating motion) and/or a rotating motion around an axis, with the proviso that the various points of said agitator or agitator assembly move at substantially the same linear speed.
  • oscillating motion e.g. a reciprocating motion
  • a particular feature of this invention is the same linear speed for each point of the agitator or agitator assembly when the latter is provided with a rotating motion around the axis, e.g. a horizontal or a vertical axis.
  • a rotating motion around the axis, e.g. a horizontal or a vertical axis.
  • the lower part of the agitator or agitator assembly is immersed within the contents of the crystallization vessel ( 1 , 2 ).
  • a rotating motion according to the present invention includes both a full rotation (i.e. 360° around the axis, clockwise and/or anticlockwise) and a more limited rotation (e.g. a pendular motion).
  • a rotating motion according to the present invention includes a rotation in such a way that each point of the agitator or agitator assembly describes a circle of substantially the same diameter in a vertical or horizontal plane.
  • substantially the same diameter is meant that the rotation about each point of the agitator or agitator assembly describes a circle in a vertical or horizontal plane whose diameter is within ⁇ 10% preferably ⁇ 5%, of the average diameter of rotation described by such a point in the agitator or agitator assembly.
  • the edible oil and fat fractionation process of the present invention is not limited to any specific type of agitator assembly construction, or to any combination of agitator motions, provided that at substantially each time of performance of the process each point of the agitator assembly moves at substantially the same linear speed.
  • the agitator assembly may be provided with an elliptic motion by combining a rotation around an horizontal axis and a vertical translation of said axis.
  • the present invention provides novel constructions of crystallizers that are suitable for industries such as, but not limited to, the edible oil or fat industry.
  • the crystallizer comprises a crystallization vessel ( 1 , 2 ), an agitator or agitator assembly, and a drive, wherein said drive provides said agitator or agitator assembly with a rotating motion around an axis, and wherein each point of said agitator or agitator assembly moves at substantially the same linear speed.
  • the crystallization vessel ( 1 , 2 ) preferably has a polygonal cross-section, especially when designed for containing edible oils and fats.
  • the crystallizer comprises a crystallization vessel ( 1 , 2 ) having a polygonal cross-section, an agitator or agitator assembly, and a drive, wherein said drive provides said agitator or agitator assembly with an oscillating motion (e.g. a reciprocating motion), and wherein said agitator or agitator assembly is not inclined with respect to the moving direction (contrary to the teaching of the prior art).
  • a crystallization vessel 1 , 2
  • the crystallization vessel 1 , 2
  • said drive provides said agitator or agitator assembly with an oscillating motion (e.g. a reciprocating motion)
  • said agitator or agitator assembly is not inclined with respect to the moving direction (contrary to the teaching of the prior art).
  • each point of said agitator moves at substantially the same linear speed. Additional optional features of these novel crystallizers are defined in the appended set of claims.
  • a crystallizer according to the invention can handle crystal slurries with a higher solid fat content (hereinafter referred as SFC) than crystallizers of the prior art, which has the great advantage that the crystallizers according to the invention can achieve in a single fractionation step, especially in a dry fractionation process for oils or fats, a result for which the prior art processes needed two or more successive fractionation steps.
  • SFC solid fat content
  • the present invention thus provides a fractionation process for edible oils and fats in a crystallizer comprising a crystallization vessel ( 1 , 2 ), an agitator or agitator assembly, and cooling means, the method comprising driving said agitator with an oscillating and/or rotating motion around a horizontal or vertical axis by a driving means, provided that each point of said agitator moves at substantially the same linear speed.
  • the cooling means may be part of the agitator or agitator assembly, or may be placed between two or more elements of said agitator or agitator assembly, or both.
  • An object of the invention to provide improved crystallization processes for edible oils and fats by using improved crystallizers.
  • An advantage of the present invention is that it can overcome at least one of the disadvantages of the fractional crystallization processes for edible oils and fats using known crystallizers.
  • An advantage of the present invention is the provision of crystallization process that can effectively be used for the fractional crystallization of a wide variety of fats and oils, and that employs a crystallization vessel displaying little hold-up of crystals upon emptying.
  • An advantage of the invention is the provision of improved crystallizers with a high cooling surface area per unit of crystallizer volume and with a design that allows this area to be increased or decreased in a manner that does not fundamentally alter the crystallizer performance.
  • An advantage of the present invention is the provision of a crystallizer with an improved heat transfer coefficient over crystallizers known in the art.
  • An advantage of the present invention is the provision of a crystallization process for edible oils and fats that allows crystal slurries to be produced that exhibit superior filtration characteristics.
  • An advantage of the present invention is the provision of a crystallization process that can be used in both solvent fractionation processes and dry fractionation processes.
  • An advantage of the present invention is the provision of a batch crystallization process for edible oils and fats making use of one or more crystallizers meeting one or more of the aforesaid improved features.
  • An advantage of the present invention is the provision of a continuous crystallization process for edible oils and fats making use of one or more crystallizers meeting one or more of the aforesaid features.
  • FIG. 1 shows the top part of a first embodiment of a crystallizer for use in fractionation processes according to the invention wherein an agitator or agitator assembly is provided with a linear, horizontal reciprocating motion.
  • FIG. 2 shows a partially cut away of a second embodiment of a crystallizer for use in fractionation processes according to the invention with an agitator or agitator assembly being provided with an oscillating motion.
  • FIG. 3 shows a longitudinal cross section through an embodiment of a crystallizer for use in fractionation processes according to the invention wherein two different types of parallel cooling elements partition the crystallization vessel into compartments and wherein the agitator or agitator assembly is positioned in between said cooling elements and is provided with a reciprocating motion.
  • FIG. 4 shows traversal cross-sections through three further embodiments of crystallizers that can be used in fractionation processes according to the invention wherein the agitator or agitator assembly is provided with (A) an oscillating motion, (B) a full rotating motion around a horizontal axis, and (C) a horizontal reciprocating motion, respectively.
  • FIG. 5 shows traversal cross-sections through two further embodiments of crystallizers for use in fractionation processes according to the invention wherein the agitator or agitator assembly is provided with a vertical reciprocating motion.
  • FIG. 6 shows the top part of a further embodiment of a crystallizer for use in the fractionation processes according to the invention wherein the agitator assembly rotates around a vertical axis.
  • FIG. 7 schematically shows a continuous fractionation process for edible oils according to the invention using a number of crystallizers in series.
  • FIG. 8 is an horizontal cross section of a crystallizer according to an embodiment of the present invention.
  • agitator means an element for agitating oils and/or fats driven by a driving means adapted to provide an oscillating and/or reciprocating and/or rotating motion so that each point of said element moves at substantially the same linear speed during said motion.
  • Parts of the driving means not meant to contact oils and/or fats but fulfilling merely the purpose of providing said oscillating and/or reciprocating and/or rotating motion to said element are not considered part of the agitator.
  • agitator assembly it relates to a set of one or more agitators as defined above, wherein each point of each agitator in the agitator assembly moves with substantially the same linear speed during a large part of its motion.
  • the agitator or agitator assembly when the agitator or agitator assembly is driven by more than one driving means, it may happen that points of the agitator or agitator assembly are moving at slightly different speed and/or are moving out of phase, so that for a short period of time, the points close to a first driving means move at a speed very different (e.g. at the time when an agitator change direction in a reciprocal movement) than points close to another driving means.
  • This situation could for instance happen in the embodiment of FIG. 5 if the pistons are operating out of phase. This would not however affect very negatively the performance of this embodiment of the present invention and most benefit of the present invention would be maintained.
  • each point of the agitator/agitator assembly moves at substantially the same speed for 80% or more, more preferably 90% or more of the time of a cycle.
  • Two linear speeds will be considered to be “substantially the same”, when their ratio is from 0.8 to 1.2, most preferably form 0.9 to 1.1.
  • Any combination of 1) time fraction range, as described hereabove, wherein the agitator/agitator assembly moves at substantially the same speed and 2) the range of speed ratio, as described hereabove, considered substantially the same are encompassed in embodiments of the present invention.
  • At least 15% of the crystallizer volume is preferably traversed by the agitator or agitator assembly during one movement cycle, with 30% or more being particularly preferred, 50% or more being especially preferred and 70% or more being particularly especially preferred.
  • the motion of the agitator or agitator assembly is such that large fluid movements within the oil or fat are reduced.
  • This relative stillness of the slurry contrasts with prior art processes in which movement of the slurry is actively sought to promote heat transfer. The relative stillness may explain the surprising observation of large crystals substantially uniform in size and morphology.
  • the crystallizer has a lack of homogeneity with respect to solid fat content of said slurry.
  • a first aspect of the present invention relates to fractionation processes for edible oils and fats making use of a crystallizer comprising a crystallization vessel ( 1 , 2 ), an agitator or agitator assembly, cooling means, and a drive, characterised in that said drive provides said agitator or agitator assembly with an oscillating motion and/or a rotating motion around an axis, such as vertical or horizontal axis, with the proviso that the various points of said agitator or agitator assembly move at substantially the same linear speed, especially when the agitator or agitator assembly is provided with a rotating motion around the said axis.
  • a crystallizer comprising a crystallization vessel ( 1 , 2 ), an agitator or agitator assembly, cooling means, and a drive, characterised in that said drive provides said agitator or agitator assembly with an oscillating motion and/or a rotating motion around an axis, such as vertical or horizontal axis, with the proviso that the various points of said agit
  • the fractionation process for edible oils or fats according to this invention may be a solvent fractionation process wherein the oil or fat to be fractionated is dissolved in a suitable solvent, or a mixture of suitable solvents, for the relevant oil or fat.
  • the fractionation process for edible oils or fats according to this invention may also be a dry fractionation process wherein the oil or fat to be fractionated is simply molten without addition of a solvent.
  • the present invention relates to a system wherein the cooling means constitute a part of the agitator or agitator assembly, or are included in said agitator or agitator assembly.
  • the present invention relates to a system wherein the cooling means are separate from the agitator or agitator assembly and wherein said cooling means comprises one or more parallel cooling elements that partition said crystallization vessel into compartments and wherein said agitator or agitator assembly is positioned in between said elements.
  • the present invention relates to a system wherein said cooling means is both part of said agitator or agitator assembly and comprises one or more parallel cooling elements that partition said crystallization vessel into compartments and wherein said agitator or agitator assembly is positioned in between said elements.
  • the agitator or agitator assembly When the agitator or agitator assembly is driven to have a combination of two or more types of motion stated above, the type of combination is not critical for the present invention.
  • the agitator or agitator assembly may be provided with an oscillating motion combined, simultaneously or subsequently, with a reciprocating motion.
  • the agitator or agitator assembly may be provided with an oscillating motion combined, simultaneously or subsequently, with a rotating motion around a horizontal axis wherein the various points of said rotating agitator or agitator assembly move at substantially the same linear speed.
  • the agitator or agitator assembly may be provided with a reciprocating motion combined, simultaneously or subsequently, with a rotating motion around a horizontal axis wherein the various points of said rotating agitator or agitator assembly move at substantially the same linear speed.
  • a reciprocating motion combined, simultaneously or subsequently, with a rotating motion around a horizontal axis wherein the various points of said rotating agitator or agitator assembly move at substantially the same linear speed.
  • the skilled person can readily design a suitable combination of motions by merely using the principles of the invention that derive from the above-described unexpected findings.
  • the crystallization vessels used in the fractionation processes according to the invention preferably have a polygonal cross-section (wherein the said polygonal cross-section preferably includes from 3 to 8 walls, more preferably from 4 to 6 walls), preferably rectangular as illustrated by FIGS. 1 and 2 or square.
  • the crystallization vessel of said crystallizer is preferably made of stainless steel.
  • said crystallization vessel can comprise relatively thin (for instance about 3 or 4 mm in thickness) rectangular walls 1 and 2 that are supported and contained by a cage construction made of mild steel sections 3 as illustrated in FIG. 2 .
  • This cage construction can also incorporate two opposite rails 4 running in the longitudinal direction of the crystallization vessel and supporting the agitator or agitator assembly as shown in FIG. 1 .
  • the crystallizer vessel is preferably provided with a feed inlet (not shown in the figures) for the starting material to be crystallised, which can be a solution or a melt, and an outlet (not shown in the figures) for the partially crystallised product resulting from operating the process according to the invention.
  • a slope of about 10 to 30 degrees (depending upon the viscosity and type of material to be crystallised), preferably about 15° with respect to the horizontal, has been found to be adequate to ensure complete emptying of the crystallization vessel by drainage.
  • Several embodiments for constructing a suitable outlet are readily available to those skilled in the art.
  • the above-mentioned slope continues right to the opposite wall of the vessel, whereas in another embodiment, two bottom halves are directed towards the centre of the crystallization vessel.
  • the vessel bottom can also be made to have a slope in its longitudinal direction to further facilitate complete emptying of the vessel at the lowest point thereof.
  • the partially cut away wall 1 of the crystallization vessel then has the shape of a rectangular trapezium.
  • the agitator or agitator assembly preferable extends to the sloping bottom so that this can also have a rectangular trapezoidal aspect.
  • the crystallization vessel walls 1 and 2 and vessel bottom, or bottom parts are preferably made from flat sheet material (e.g. stainless steel sheets).
  • a bottom that is curved in one direction and that can therefore also be constructed from a flat sheet constitutes another embodiment of the crystallization vessel to be used in the fractionation process according to the invention.
  • the crystallizer to be used in the fractionation processes for edible oils and fats of this invention is preferably provided with a lid (not shown in FIGS. 1 and 2 ) in order to prevent dirt from falling into the product being crystallised and/or to thermally insulate this product from its environment.
  • This lid does not need to support any heavy auxiliary equipment like an agitator, so its construction can be quite light.
  • the lid is preferably provided with sight-glasses and appropriate lighting. If the crystallizer is used in a solvent fractionation process according to the invention, the lid should preferably be sufficiently air tight to retain the solvent inside the crystallization vessel.
  • the agitator or agitator assembly itself acts as a heat exchanger and comprises a conduit for a heat exchange medium that is connected to an inlet and an outlet for said heat exchange medium.
  • the crystallizer also comprises a drive, and according to the invention, each point of said agitator or agitator assembly moves at substantially the same linear speed when put in motion by said drive.
  • FIGS. 2 and 3 schematically show non-limiting embodiments of approach (A).
  • Another approach (B) comprises stationary heat exchange elements (i.e. elements able to cool the molten or dissolved edible oil or fat) that may entail the partitioning of the crystallizer (i.e. the crystallization vessel) by hollow elements acting as heat exchangers.
  • Said hollow elements may comprise flat, double-walled heat exchangers that have been provided with an internal labyrinth or a series of parallel hollow tubes.
  • FIG. 3 Two embodiments of approach (B) have been illustrated in FIG. 3 that also shows how the elements of the agitator or agitator assembly may be positioned in between these partitioning heat exchange (i.e. cooling) elements.
  • both the partitioning elements and the agitator or agitator assembly act as heat exchangers.
  • a lower cooling rate is generally preferred, so that approaches (A) and (B) are generally most suited.
  • Approach (B) comprising stationary heat exchange (i.e. cooling) elements will in general provide a lower heat transfer coefficient than approach (A), a difference which can suitably be compensated by correspondingly adapting the cooling surface area.
  • the non-stationary cooling surface of approach (A) is often preferred for crystallizers operating in a continuous fractionation process, e.g. a continuous dry fractionation process, since they minimise the risk of incrustation.
  • agitator or agitator assembly all points of which move according to the invention, at substantially the same linear speed when put in motion by the drive can be executed in various ways without departing from the principles underlying the present invention.
  • rails 4 are provided close to or on the top of opposite longitudinal walls 1 of the crystallization vessel and act as a support for the agitator assembly.
  • This assembly comprises a rectangular steel frame having longitudinal portions 5 to which one or more wheels 7 have been fastened, and transverse portions 6 parallel to the transverse walls 2 of the crystallization vessel. These wheels 7 allow the agitator or agitator assembly to be provided with a reciprocating motion along rails 4 .
  • the steel frame ( 5 , 6 ) also supports a conduit for a heat exchange medium.
  • An embodiment of such a conduit as illustrated in FIG. 1 comprises two hollow headers 8 and 9 that are parallel to rails 4 and are connected to the frame ( 5 , 6 ).
  • the hollow header 8 is connected to a supply source (not shown) of the heat exchange medium, usually water, and the other hollow header 9 is connected to a heat exchange medium return inlet (not shown). Both connections of the hollow headers 8 and 9 should preferably be flexible enough to allow the agitator assembly to move along rails 4 .
  • the two hollow headers 8 and 9 are connected to each other by a series of hollow distributors 10 and 11 in such a way that the hollow distributor 10 is connected to the cooling medium supply header 8 and only supported by the hollow header 9 , whereas the hollow distributor 11 is connected to the hollow header 9 and only supported by header 8 .
  • the hollow distributors 10 and 11 are connected to each other by U-shaped tubes 12 that extend down to the bottom of the crystallization vessel and ensure proper heat exchange.
  • the heat exchange medium (usually water) thus flows from the hollow header 8 into the first or any odd-numbered hollow distributor 10 , through U-shaped cooling tubes 12 , into odd-numbered hollow distributors 11 , to be collected by the hollow header 9 that is connected to the heat exchange medium return system.
  • Orifice plates can be inserted in the connections between the hollow distributor 11 and the hollow header 9 to ensure that the system is completely filled with heat exchange medium and that the flow rate of said heat exchange medium through each tube or hollow section is approximately the same.
  • the U-shaped cooling tubes can be connected to each other at some lower point to provide rigidity to the agitator or agitator assembly.
  • Rails 4 allowing motion of the agitator or agitator assembly are preferably not immersed into the oil or fat being crystallised.
  • the hollow headers 8 and 9 are preferably located below the surface of the crystal-containing slurry. Otherwise moisture from the air may condense on these hollow headers, fall down and contaminate the product being crystallised.
  • FIG. 2 shows another embodiment of an agitator or agitator assembly according to approach (A) of the present invention.
  • the transversal portions 6 of the rectangular steel frame are connected via swivels 13 to stationary bars 14 that are connected to the walls 1 of a rectangular or square-shaped crystallization vessel.
  • a further stationary bar 15 supports a piston 16 that is also attached to the transverse frame portion 6 . Movement of the piston 16 provides the agitator or agitator assembly, comprising hollow headers 8 and 9 , hollow distributors 10 and 11 and U-shaped tubes 12 attached to the frame ( 5 and 6 ), with an oscillating motion in such a way that all points of said agitator or agitator assembly move at substantially the same linear speed.
  • a crystallizer according to the present invention preferably has a cooling surface in the range of about 2 to 10 m 2 /m 3 , more preferably about 4 to 6 m 2 /m 3 .
  • this can easily be achieved by incorporating for instance some 15 U-shaped tubes of 50 mm diameter per square meter of surface of the crystallization vessel. Attaching the U-shaped tubes at 100 mm intervals to the hollow distributors 10 and 11 , and spacing the latter at some 350 mm distance achieves the above stated range for the cooling surface.
  • it provides a sturdy assembly that can easily be moved as a whole even when the U-shaped cooling tubes 12 have been made by bending 6 m long tubes.
  • This example relates to a standard ex-factory length which is commensurate with an industrial crystallizer according to the invention of some 3 m height.
  • the rigidity of the assembly shown in FIG. 2 can also be further ascertained by connecting the cooling tubes 12 to each other at some lower point.
  • connection points of the U-shaped cooling tubes 12 to the hollow distributors 10 and 11 can be but need not be staggered. Staggering constitutes a preferred embodiment since it increases the heat transfer coefficient of the crystallizer used in fractionation processes according to the invention. However, the invention is not limited to this embodiment.
  • Approach (B) is illustrated by a longitudinal cross section through an embodiment of a crystallizer in FIG. 3 .
  • the partitioning elements may be double-walled dividers 17 as shown on the right hand side of FIG. 3 . or horizontal tubular heat exchangers 18 as shown on the left hand side of FIG. 3 ; these tubes may also be positioned vertically.
  • a distance of about 40 cm between these dividers 17 or 18 also ensures a cooling surface of some 5 m 2 per m 3 of the crystallization vessel. This distance is sufficient for enabling a rotating motion of agitator elements 19 .
  • This rotating motion can be around a horizontal axis as illustrated schematically in FIG. 4B or around a vertical axis as illustrated by FIG. 6 .
  • Increasing the distance between dividers 17 or 18 to about 50 cm decreases the cooling surface to 4 m 2 /m 3 , a value which is still within the preferred range of this invention.
  • each agitator element 19 is shaped like a gate. It can be attached to pistons 20 that provide the agitator with a reciprocating vertical motion. In another embodiment it can be attached via swivels to a device (such as, but not limited to, a crankshaft, or alternatively eccentric wheels 21 as shown in FIG. 4B ) whereby the gate-shaped agitator elements can be attached to each other by frame portion 22 to form an agitator assembly.
  • a device such as, but not limited to, a crankshaft, or alternatively eccentric wheels 21 as shown in FIG. 4B
  • the agitator assembly is provided with a rotating motion around a horizontal axis whereby all points of said agitator assembly move at substantially the same linear speed. Wheels 21 can also be used to provide the agitator with an oscillating motion if so desired.
  • Another embodiment according to approach (B) comprises partitioning elements comprising a series of parallel, vertical hollow tubes through which the cooling medium flows.
  • This medium can for example be fed via a mains that is situated in a bottom corner of the crystallization vessel and parallel to its longitudinal direction, and that is connected to a series of horizontal distributor pipes that are perpendicular to the mains.
  • Each horizontal distributor pipe can then feed a series of parallel, vertical cooling tubes.
  • These tubes are then connected to a series of collectors whereby these connections may comprise orifice plates to ensure an even distribution of the cooling medium through the cooling tubes.
  • the heat exchange partitioning elements preferably have the cooling medium fed at their lowest point especially when the crystallizer is used in a continuous fractionation process according to the invention, but the invention is in no way limited to this embodiment.
  • FIG. 6 Yet another embodiment of a crystallizer to be used in the process according to the invention is shown in FIG. 6 . It illustrates a rectangular crystallization vessel with walls 1 and 2 that is surrounded by mild steel sections 3 that also comprise horizontal bars 23 above the vessel. Extending downward from bars 23 are a number of supports 24 , the lower ends of which are provided with a circular disc 25 that is attached to the support 24 by a ball bearing in the centre of the disc 25 . Further supports 26 are attached eccentrically to discs 25 and a crossbar 27 is attached to the supports 26 .
  • the agitator assembly 28 is attached to crossbars 27 and when one of the discs 25 is made to rotate by drive 29 , the whole agitator assembly 28 will rotate around a vertical axis whereby each point of said agitator assembly 28 moves at substantially the same linear speed.
  • drive 29 could also be a piston so that the resulting periodic motion of agitator assembly 28 will be an oscillating motion around a vertical axis.
  • FIG. 8 Yet another embodiment of a crystallizer according to the present invention is displayed as a horizontal cross section in FIG. 8 .
  • Cooling water enters the supply header 8 at the left top corner of the drawing which header feeds distributors 10 .
  • the U-shaped cooling tubes 12 are indicated in the drawing by circles that are connected by straight lines indicating the top view of U-shaped cooling tubes 12 .
  • the water flowing through the cooling tubes 12 is collected by distributors 11 that are connected to header 9 from which the water flows to the cooling unit as shown on the top right hand side of the drawing.
  • the dotted lines in the drawing indicate the areas the cooling tubes 12 traverse when the agitator assembly is moved to and from in a reciprocating manner.
  • fitting the cooling tubes 12 to the distributors 11 in such a way that the plane containing the central axes of the two vertical portions of a cooling tube 12 is at an angle to the direction of said movement increases the area of the crystallizer being traversed by the cooling tubes 12 .
  • the motion of the agitator or agitator assembly can also be a reciprocating motion in a horizontal plane as illustrated in FIG. 1 and FIG. 4C wherein for instance a double piston drive ensures this type of motion.
  • This embodiment of the invention is not limited to using a double piston drive, and an electrically driven rotating motion that is converted into a reciprocating motion is also within the scope of the invention.
  • the double piston drive embodiment has been found effective and adequate by ensuring a reliable operation of the crystallizer and by requiring little maintenance.
  • an amplitude of agitation of about 20 to 100 cm, preferably about 30 to 50 cm, and/or a frequency of agitation of about 5 to 50 min ⁇ 1 , preferably about 15 to 30 min ⁇ 1 have been found suitable to ensure a proper heat transfer in most situations and to generate fat crystals that can be easily separated from their mother liquor.
  • the agitator or agitator assembly can also be moved up and down within a vertical plane as shown in FIG. 3 and FIG. 5 .
  • FIG. 4B A combination of these two types of motions is shown in FIG. 4B where the agitator assembly rotates around a horizontal axis; this embodiment can be suitably performed e.g. by attaching the agitator to a crankshaft or eccentrically to wheels 21 .
  • the agitator motion is preferably a reciprocating motion in a vertical direction as illustrated by FIG. 3 and FIG. 5 , or a rotating motion around a horizontal axis as illustrated by FIG. 4B .
  • the agitator motion can also be a reciprocating motion in a horizontal direction as shown in FIGS. 1 and 4C , a rotating motion around a horizontal axis as shown in FIG. 4B , or a rotating or oscillating motion around a vertical axis as shown in FIG. 6 .
  • a horizontal reciprocating motion parallel to the partitioning elements has also been found to be an effective way of agitation when applied to the crystallization of oils and fats. Combinations of these various periodic motions also fall within the scope of the present invention.
  • FIGS. 3 and 5 show a drive comprising two pistons.
  • the two pistons can also operate slightly out of phase without departing from the present invention.
  • the agitator gate will be slightly tilted in an anti-clockwise direction when the pistons are both moving down. After piston 20 A has reached its lowest position, it moves upwards again while piston 20 B is still moving downwards. This causes the agitator assembly to rotate in a clockwise direction around a horizontal axis.
  • the agitator or agitator assembly When the agitator or agitator assembly is moved in accordance with the invention, it exerts no net lifting force onto the surrounding slurry so that any crystals the latter contains can easily settle, said crystals having a higher density than oil.
  • crystals settling is not damaging for fractionation results. If nevertheless the avoidance of crystal settling would be desirable in a specific situation, crystals settling can be effectively avoided by fitting the agitator or agitator assembly with hinged scoops that lift the crystal material when the agitator moves in one direction but do not force it down when the agitator moves in the reverse direction.
  • the fractionation process according to any of the above-described embodiments of the invention is eminently suitable for the batch dry fractionation of edible oils and fats such as, but not limited to, palm oil.
  • molten oil or fat is introduced into the crystallization vessel and, if any residual crystals stayed behind from the previous batch, these residual crystals easily melt so that a homogenous starting material results.
  • the preferably homogeneous starting material can then be subjected to a cooling regime that may however be preceded by a heating step to erase any crystal memory still present, and comprises one or more gradual cooling periods and possibly one or more temperature holding periods.
  • the number of cooling periods, the cooling rate of each said cooling period, and the duration of each temperature holding period, if any, are not critical to the batch fractionation process of the present invention, and can be determined for each type of oil or fat based on the standard knowledge of the person skilled in the art.
  • the final batch temperature determines both the olein properties and the amount of crystals produced when equilibrium is reached.
  • the fractionation process may also be stopped before equilibrium has been reached so that more crystals may be formed in the slurry awaiting the subsequent separation step.
  • the resulting crystal slurry may be held in the crystallization vessel during a waiting stage, but it may also be dropped from the crystallization vessel into one or more intermediate storage vessels serving for feeding the separation equipment of the subsequent separation step.
  • An agitator of a type standard in the art is preferably fitted to this intermediate storage vessel to prevent the crystal slurry from settling before it enters the separation equipment.
  • each of a number of crystallization vessels is filled in turn with the material, e.g. the oil or fat, to be crystallised, and when each batch has been crystallised to the desired extent, the contents of each crystallization vessel can then be dropped into an intermediate storage tank.
  • the separation equipment used for separating crystals from their mother liquor can be of any type known in the art, i.e. it can be suitable for continuous operation but it can also be suitable for batch-wise operation.
  • the crystallizer according to any of the above-described embodiments of this invention is also suitable for performing a continuous fractionation process of oils and fats, as illustrated in FIG. 7 .
  • the oil feed stream is first heated and kept in a holding vessel where crystal memory is erased. Because the process is continuous, the energy requirements of the heating and subsequent cooling can be reduced by the use of economisers.
  • the number of crystallizers in series in the continuous fractionation process according to the invention can be three as shown in FIG. 7 as a well-performing but non-limiting example, but more or fewer crystallizers can be used as well to meet special fractionation requirements.
  • the first crystallizer can also be used to cool the oil feed stream to about 3 to 8° C.
  • this cooling is preferably effected in a heat exchanger upstream from the first crystallization vessel as shown in the top right portion of FIG. 7 , for instance a heat exchanger of the tube and shell type well known in the art. Because of the final product temperature aimed for, there is no risk of crystal deposition inside this heat exchanger provided that the temperature difference between the oil product and the coolant (e.g. water) is not too large i.e. less than 1° C.
  • the coolant e.g. water
  • Each crystallizer used in the continuous dry fractionation process according to the invention comprises a crystallization vessel.
  • the latter comprises a feed inlet that is preferably constructed in such a way that the feed hardly mixes with the vessel contents and remains floating on top of said contents.
  • horizontal sheets may be provided onto which the feed stream is directed through a multitude of mouths and from where the feed stream flows horizontally into the crystallization vessel, just like cream is spread on top of an Irish coffee by pouring it slowly on the backside of a spoon. Said horizontal sheets are therefore preferably located just below the vessel content surface and they can be conveniently attached to the agitator.
  • Each crystallization vessel used in the continuous dry fractionation process according to the invention also comprises an outlet that collects material from the lowest part of said vessel.
  • a possible way of controlling the liquid (mother liquor) level in said vessel is by connecting said outlet to a mounting tube that is connected to a bend at the desired level. When then the crystallization vessel is filled, the liquid level in said tube rises until the material starts to overflow into a downstream crystallizer and thus maintains the liquid level at a fixed position.
  • the diameter of said mounting tube must be sufficiently narrow so that the flow rate inside said tube is able to entrain any crystals possibly entering said tube, but not so narrow as to cause a large difference in height between the bend in the tube and the liquid level in the crystallization vessel. Designing the appropriate tube diameter by taking both conflicting requirements into account is within the general knowledge of the person skilled in the art.
  • the lifting of crystals due to agitator motion is preferably avoided. Accordingly, vertical movement inside the crystallization vessel is preferably minimised. This further allows the highest temperature gradient inside the crystallization vessel to be maintained and permits the use of the lowest possible number of crystallization vessels in series.
  • the last of the crystallizers in series (the third crystallizer shown in FIG. 7 ) is connected to either a continuously operated separator or to an intermediate storage vessel feeding a discontinuously operated separator like a membrane filter press (not shown in FIG. 7 ).
  • the cooling medium e.g. water
  • the cooling medium is preferably used in counter-current to the stream of material being crystallised, e.g. (with reference to FIG. 7 ) with water leaving the third crystallizer feeding the second crystallizer, and so on.
  • the cooling medium (e.g. water) circuit of each crystallizer is preferably provided with independent temperature control means, e.g. by injecting cold water into the cooling water stream.
  • RBD bleached and deodorised palm oil with an iodine value (hereinafter referred as IV) of 52.7
  • RBD bleached and deodorised
  • IV iodine value
  • the rectangular crystallization vessel is 80 cm high, 45 cm wide and 100 cm long.
  • an agitator suitable for horizontal motion was fitted as shown in FIG. 1 .
  • the agitator comprises two sets of 5 U-shaped tubes each assembled together. These tubes (diameter 33 mm) extend almost down to the bottom of the crystallization vessel. Accordingly, the cooling surface is about 2 m 2 and the cooling surface to volume ratio is about 5.6 m 2 /m 3 .
  • the crystallization vessel was filled with molten RBD palm oil that was then heated to 70° C. over a period of 30 minutes and held at that temperature for 15 minutes to erase any crystal memory. Cooling parameters used during each step of the RBD palm oil crystallization process are reported in table 1 below.
  • Table 3 shows SFC values of slurry samples and IV values of olein samples taken at different levels of the crystallization vessel after two different steps of the crystallization process.
  • step 5 SFC at top of vessel 14.2 29.8 SFC at intermediate level 18.1 29.1 SFC at bottom of vessel 21.0 28.5 IV slurry at top of vessel 53.05 52.77 IV slurry at bottom of vessel 52.11 52.93 IV olein at top of vessel 59.22 62.87 IV olein at bottom of vessel 59.20 63.04
  • a commercial palm olein with an IV of 57.7 was used as raw material. If this olein is used as such, the crystal slurry produced by cooling the olein is already quite viscous when its SFC is still only 16% by weight. Filtering this viscous slurry by using a membrane filter press yields a filter cake with an SFC of only 38% by weight at a cake thickness of 50 mm. The SFC of the cake can be increased to 45% by weight when the cake thickness is reduced to 25 mm but in both cases the IV of the olein was only 61.5.
  • a much higher olein IV can be obtained by improving crystallization by adding 8% by weight of palm oil to the palm olein before this is heated to 60° C. and then cooled in the crystallizer according to the invention and as used in Example 1.
  • the resulting slurry had an SFC of 24.3% by weight after having been cooled down to 14° C. over a period of 13 hours and yielded 60% by weight of an olein with an IV of 65.4.
  • the corresponding stearin fraction had an IV of 46.6.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)
US12/175,837 2006-01-20 2008-07-18 Fractionation processes and devices for oils and fats Active 2029-07-22 US8203014B2 (en)

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EP06001195.4 2006-01-20
EP06001195 2006-01-20
EP06001195A EP1818088A1 (en) 2006-01-20 2006-01-20 Crystallisers useful in fractionation processes for oils and fats
PCT/EP2007/000499 WO2007082766A1 (en) 2006-01-20 2007-01-22 Fractionation processes and devices for oils and fats

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GB2449572A (en) 2008-11-26
US20090264667A1 (en) 2009-10-22
SE533074C2 (sv) 2010-06-22
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MY146759A (en) 2012-09-14
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